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OPERATING INSTRUCTIONS

FOR
DIGITAL AUTOMATIC KARL FISCHER TITRATION APPARATUS,
MODEL: VEEGO/MATIC-MD.

I] INTRODUCTION

VEEGO/MATIC-MD, is a Microprocessor Based Automatic Karl Fischer Titrator,


designed for accurate estimation of moisture in various samples. It is based on
Volumetric Principle.

II] DESCRIPTION OF THE INSTRUMENT

The base of VEEGO/MATIC-MD, incorporates an electronic circuitry and a magnetic


stirrer. A four line LCD display, ON/OFF switch, (stirrer speed controller) and a feather
touch keyboard are provided on the front panel.

III] CHECK AND IDENTIFY FOLLOWING PARTS SUPPLIED


WITH THE INSTRUMENT:

01) Main Unit, Model: VEEGO/MATIC-MD. -- -- -- 1 No.


02) Reservoir Bottles. 250 ml/-each. (Amber coloured) -- -- 2 Nos.
03) Ground glass adapter for reservoir. -- -- -- 2 Nos.
04) Ground glass stopper for reservoir. -- -- -- 1 No.

05) Calcium Chloride/Silica Gel Bulb with ground


glass joint. (Moisture trap) for reservoir. -- -- -- 2 Nos.

06) Moisture Beaker with ground edge. -- -- -- 1 No.

07) Adjustable clamp for moisture beaker with pair of


Bakelite nuts, tightening key, one large rubber cork
and a beaker holding ring with two screws fitted. -- -- 1 No.

08) Magnetic Stirring Rotor. -- -- -- -- -- 1 No.


09) Stainless Steel Support Rod with Tightening Key. -- -- 1 No.
10) Pt-Sensors. (Electrodes) -- -- -- -- -- 2 Nos.
11) Glass Funnel. -- -- -- -- -- -- 1 No.
12) Small Box Spanner. (Nut driver) -- -- -- -- 1 No.
13) Silicon Tube (Std.Length) for dispenser pump. -- -- 4 Nos.
14) Black rubber coupling tube. -- -- -- -- 12 Pieces.
15) Teflon Tube. -- -- -- -- -- -- 3 Pairs.

16) Instruction Manual. -- -- -- -- -- 1 No.

1
CONTROLS ON THE PANEL

3.1) A mains switch is provided on the front panel. This switch puts the instrument
`ON' and FOUR line LCD screen will glow.

3.2) A stirrer speed controller is provided to adjust the desired stirrer speed.

3.2) A keyboard having 16 keys is provided on the front panel. The numeric
keypad consists of 0 to 9 keys along with a decimal key. These keys are used
to enter values of sample, density etc. The other keys are-

3.3/1) START On pressing this key, the titration starts.

3.3/2) CAL I These keys are to be pressed for standardizing or calibrating


& CAL IT K/F Reagent.

3.3/3) CLEAR On pressing this key, the present message on the display gets
clear and sign `ON’ message appears.

3.3/4) ENTER This key is pressed after entering the value of sample, density etc.

3.3/5) 0 ----- To select the function (CONT./END/CLEAR) while calibrating the


SELECT K/F Reagent.

3.3/6) 1 BATCH To enter the batch no.


NO

3.3/7) 2 SET To set the current time and date.

CLOCK
3.3/8) 3 PRINTER On pressing this key, the printer will print all the necessary
data related to the sample under test.

3.3/9) 4 EX TIME To adjust the stirring time for extraction of moisture from
sample (1 to 240 seconds).

3.3/10) 5 Solvent To enter the blank reading of solvent if the sample is diluted with
Blank a solvent.

3.3/11) 6 FACTOR This key is used to enter the strength of K/F Reagent i.e. the
factor of K/F Reagent.(The capacity of reagent to absorb
moisture)

2
3.3/12) 7 % On pressing this key, the display shows percentage, PPM
PPM and milligrams of moisture present in the sample.

3.3/13) 8 DENSITY This key is used to enter the density of liquid sample added.

3.3/14) 9 SMPL This key is used to enter the weight or volume of the sample
QUANTITY added in grams or milliliters.

3.3/15) CE This key is used to cancel the entered value.

3.3/16) * CLEAN This key is used for cleaning operation.

IV] SETTING UP THE INSTRUMENT

4.1) Before proceeding to assemble the parts, it is absolutely essential that reservoir,
beaker, adapter are perfectly free from moisture. DO NOT clean them with
water. Rinse the reservoirs and moisture beaker with methanol and dry them
well before use. They may be washed with water, if sufficient time can be
allowed for drying in an oven.

4.2) Proceed to assemble the unit as under:

4.2/1) Fix the reservoir housing in the clamp provided on the rear Plate of the main
instrument by just sliding them. Fit the two Reservoirs in the holders provided
on the housing.

4.2/2) Fit the adapter to the left hand side reservoir and the plain stopper to the other.

4.2/3) Two Teflon tubes are fitted to the dispenser unit, with black coupling tubes.
The right hand side tube marked as outlet is fitted to a Teflon nozzle. This
nozzle should be attached to the beaker assembly. Attach the nozzle to the left
hand side hole at rear on the Teflon cover. The left hand side tube of the
dispenser marked as inlet should be attached to the adapter of the reservoir.

4.2/4) Apply carefully good quality grease to the ground edge of the moisture beaker
and fit the beaker to the adjustable clamp with the help of the ring having
screws. Do not tighten the Bakelite nuts excessively.

4.2/5) Fit the support rod in socket provided on the instrument at the rear. Fit the
clamp with the moisture beaker to the support rod. Bottom of the beaker
should be just touching the circular stirring table disc on the instrument.

4.2/6) Insert the two Pt-Sensors in the two holes of Teflon cover of the clamp. The
two holes for holding the sensors are having soft black bushes. Adjust the
sensor height such that wire tips are about 1" clear from bottom of the beaker.

3
4.2/7) Put some calcium chloride or silica gel as drying agent in the bulb of the
moisture trap. Mount the moisture trap on the adapter of the reservoir.

4.2/8) Following chemicals should be used for K/F Titration’s and are available of
well-known manufacturers. It is necessary that these chemicals are fresh.

1. Pack of K/F Reagent.

2. Methanol of special K/F grade having moisture contents less than 0.05%.

3. Sodiumtartrate-di-hydrate special K/F grade. (OR Microlitre Syringe.


Capacity: 25 Microlitres.)

IMPORTANT:
While applying grease utmost care should be taken so that the tips of the electrodes
and side wall of moisture beaker, do not come in contact with grease. Always use only
special quality vacuum grease.

4.3) Add as per requirement K/F Reagent in the reservoir bottle fitted with the
adapter. (i.e. Left Hand Side Reservoir)

Needless to state that the glassware used should be well dried, otherwise
reagent will become faulty before use.

4.4) Remove the large rubber cork and add some K/F grade Methanol to the reaction
beaker to such an extent that the metal wires of sensors in the beaker are fully
immersed. Replace the cork immediately.

4.5) Connect the leads of the Pt-Sensors to the sockets provided on the instrument.

4.6) Connect the Titrator to mains supply and put the mains switch `ON'. The four
line LCD display will `GLOW'. Adjust the speed of the magnetic stirrer such that
the sensor wires do not get exposed to air. The height of the sensors in the
beaker should be so adjusted (as explained earlier) that the magnetic rotor does
not hit them while rotating.
Note: The K/F Reagent & Methanol are highly Hygroscopic. Expose
them to atmosphere for minimum time and store them always
well stoppered.

** THE TITRATOR IS NOW READY FOR GOING IN OPERATION.

4.7) The display will indicate.

VEEGO INSTRUMENTS
CORPORATION

KARL FISCHER TITRATOR

4
The message will remain `ON' for few seconds and will change to-

VEEGO/MATIC MD

16:20:11 13/08/00

V] TO SET THE CURRENT TIME AND DATE.

5.1) As seen in the above display second line of the display shows real time and date
(which are arbitrary depending on last check and figures taken for example).

5.2) For clock settings, press SET CLOCK key.

The following message or any previous stored values will appear on the screen.

The `Time' message will keep on flashing.

TIME : HR : MIN : SEC


00 00 00

DATE : DD / MM / YY
00 00 00

To set the clock, for example 10 : 15 : 24, press [1] [0] [1] [5] [2] [4]

and press ENTER key.

The screen will appear as under and `DATE' message will start flashing.

TIME : HR : MIN : SEC


10 : 15 : 24

DATE : DD / MM / YY
00 00 00

Now to enter the date, for example 13/11/00, press [1] [3] [1] [1] [0] [0]

and press ENTER key.

5
The screen will appear as-

TIME : HR : MIN : SEC


10 : 15 : 24

DATE: DD / MM / YY
13 / 11 / 00

Then press ENTER key.

The screen will appear as-

VEEGO/MATIC-MD

10 : 15 : 24 13/11/00

VI] OPERATION:

Karl Fischer Titration’s are carried out in three stages.

1st to neutralize methanol added to moisture beaker as solvent.

2nd to find out titre factor.

3rd to test the sample.

TO OPERATE, PROCEED AS UNDER:

6.1) Press START key.

The message will appear as-

Add Sample

Ex. Time = 10 secs.

6
6.2) The 4th line shows the stirring time (the set stirrer time is 10 secs, this time can
vary from 1 sec to 240 sec). When the set stirring time decrements to `00'.

The display will indicate-

Add sample

Ex. Time `00'

6.3) Then dispensing unit will start adding K/F Reagent into the beaker through
delivery tube.

The display will indicate as-

TITRATION STARTED
00 : 01 ml
EXCESS WATER
Conf. Time : 20 Secs.

6.4) 2nd Line: of the display indicates the consumption of K/F Reagent in ml.
Initially, the dispensing tubes are not filled with the reagent, but the counts will
start increasing. Once the tubes are filled with the reagent, then the reagent
will start entering in the titration vessel. Naturally, this reading of reagent
should be ignored.

3rd Line: Indicates the presence of moisture. i.e. `Excess Water’.

4th Line: of the display indicates the end point duration. The end point should
last for 20 secs. When the time counts down to `00', it indicates the end point
is reached.
6.5) NOTE: When the addition of K/F Reagent is in progress, the counts will
increase, elapse time will indicate 20 secs. When the addition of K/F Reagent
stops, the time will start decrementing. Excess water message will disappear. If
the moisture still exists in the titration vessel, even after time counts down to
`00', the addition of K/F Reagent will continue again. The counts will
increment Excess water message will appear and the elapse time will indicate
20 secs. again. When the total moisture is neutralized, the addition of K/F
Reagent and the counting will stop, the elapse time will count down to `00'
excess water message will disappear and audio signal will indicate titration is
over.

7
6.6) This display will change to-

K/F REAGENT READING

06.52 ml

6.6) To make titration vessel moisture free, follow the above procedure (i.e. para
6.1) 2 to 3 times.

This indicates that the methanol is neutralized (or titration vessel is moisture
free) and 1st stage of titration is over.

6.7) To find out Titre factor.

6.7/1) Procedure- Press CAL key and add 10 ul (microlitre, i.e. 10 mgs) of distilled
water in the titration vessel.

The display will indicate-

Add 10 MICRO LIT


Distilled water
and
Press Enter.

Press ENTER key.

6.7/2) The display will indicate-

CAL IN PROGRESS
00 : 00 ml.
EXCESS WATER
Conf. Time : 20 sec.

6.7/3) The 3rd line indicates the extraction vessel contains moisture indicated as
excess water.

6.7/4) 2nd line of the display indicates the consumption of K/F Reagent to neutralize
the 10 mgs of moisture added into titration vessel. When the addition takes
place, the counts starts increasing.

6.7/5) 4th line of the display indicates the time duration of end point. After
the completion of titration if the end point exits for 20 secs, it indicate the
titration is over.

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6.7/6) Even then if some moisture still exists after the time count downs to `00’, the
dispensing unit will start adding in the titration vessel and counts will increase.

6.7/7) The message appearing on the will be

CAL. IN PROGRESS
01 : 50 ml

Conf. Time : 20 secs

6.7/8) When the total moisture is neutralized, the message `EXCESS WATER’ will go
`OFF’ , confirmation time count down to `00’, the counts of reagent will
increase accordingly and the end point will be indicated by audio signal.

6.7/9) The message will appear as-

CAL. IN PROGRESS
02 : 25 ml.

CONF. TIME : 00 Secs.

6.7/10) After the audio signal, the message will appear as-

K/F Reagent Reading = 02 : 25 ml.

6.7/11) The above message will remain for few seconds


and message will change over to-

6.7/12) Factor = 04 : 4444


K/F READING =r 02 : 25 ml.
Repeat New factor ? ?
CONT. / END / CLEAR.

`CONT’ message is flashing.

9
6.7/13) NOTE

[`CONT’ (Continue) message is flashing. (`CONT’ = If one wants to repeat


the test (i.e. to verify titre factor, press ENTER key) when `CONT’ message is
flashing.]

If `Select’ key is pressed, `END’ message will start flashing.


(`END’ = If one wants to stop calculating titre factor, press ENTER key when
this message is flashing.

If `SELECT’ key is pressed again, clear message will start flashing.


(`CLEAR’ = If one wants to clear the existing K/F Reagent reading and titre
factor, press ENTER key, the readings will get cleared and `CONT’ message
will start flashing.]

6.7/14) If one wants to verify factor (i.e. second time)

press ENTER key, the

6.7/15) the message will appear as-

Add 10 Microlitre
of distilled water
and
Press Enter

Press ENTER key.

6.7/16) The display will indicate as-

CAL. IN PROGRESS
00 : 00 ml
EXCESS WATER
Cont. Time = 20 Secs.

6.7/17) The above message will remain `ON’ for few seconds and will change over to-

Wait Calculating Factor

6.7/18) The above message will remain `ON’ for few seconds and will change over to-

Factor = 04.4444
K/F READING = 02:25 ml
REPEAT NEW FACTOR ?
CONT. / END / CLEAR.

10
6.7/19) `CONT’, message is flashing. If one wants to `CLEAR’ the above reading,
press `SELECT’ key, then `END’ message will start flashing. Again press
`SELECT’ key, `CLEAR’ message will start flashing. If `ENTER’ key is
pressed again, the reading and factor value will be cleared.

6.7/20) The message will appear as-

FACTOR CLEARED

REPEAT NEW FACTOR ?


CONT. / END / CLEAR

6.7/21) And `CONT’ message will start flashing. If one wants to find repeat factor,
press ENTER key.

6.7/22) And follow the procedure as per paragraph no:6.7/1 to 6.7/12.


6.7/23) User can clear as many readings he wishes and he can take average of six
factor.

6.7/24) After calculation of sixth factor, for example-

The display will appear as-

Factor = 05.0000
K/F Reading = 02:00 ml.
REPEAT NEW FACTOR ?
CONT. / END / CLEAR

This display will remain for few seconds.

6.7/25) And will change over to-

WAIT
CALCULATING AVERAGE
FACTOR

The above message will remain for few seconds,

6.7/26) And will change over to-

Av. Factor =

PRESS ENTER TO CONT.

11
6.7/27) When ENTER key is press, the message will appear as-

VEEGO/MATIC-MD

17 : 06 : 09

6.7/28) If user wants to calculate only average of three titre factors, for example,

The message appearing on the display after three tests is-

Factor = 05 : 2632
K/F READING = 01 : 10 ml.
REPEAT NEW FACTOR ?
CONT. / END / CLEAR.

`CONT’ message is flashing.

6.7/29) Press 0 ------ key.


SELECT

`END’ message will start flashing.

Press ENTER key.

6.7/30) The message will appear as-

WAIT
CALCULATING AVERAGE
FACTOR

the above message will remain for few seconds,

6.7/31) and will change over to-

Av. Factor =

Press ENTER to cont.

6.7/32) Press ENTER key.

12
The message will appear as-

VEEGO/MATIC-MD

17 : 13 : 37

VII) FACTOR KEY. 6 FACTOR

7.1) When the reagent is calibrated (i.e. Titer Factor) by using CAL key, the reading
of titer factor goes in memory.

To see the reading if necessary, press FACTOR key.

7.2) The same key i.e. factor key can be used to enter the titer factor manually, if
desired.

7.3) As an example, press FACTOR key, the display will appear as-

K.F. REAGENT FACTOR

05.0000 mgs/ml

PRESS ENTER TO CONT.

(The figure displaying on the screen taken for example.)


7.4) (Suppose if one wants to enter the titer factor which is manually calculated by
way of pressing `START’ key and adding known quantity of moisture).

Such as Titer factor = 6.25

Press [6] [*] [2] [5] keys.

7.5) The display will appear as-

K.F. REAGENT FACTOR

0006.25 mgs/ml.

PRESS ENTER TO CONT.

Press ENTER key.

13
7.6) The display will appear as-

K.F. REAGENT READING

01.40 ml

(The second line may be of last test).

VIII] IIIrd Stage.

8.1) TO TEST THE SAMPLES.

Example: Powder Sample = Suppose powder contain 12% moisture.


Sample Quantity = (150 mgs = 0.150 gms) taken for example.
(Obviously, the sample will contain 18 mgs of H2O which the instrument
should evaluate).

(Hint: If the moisture is high, the sample quantity should be taken less.
If the moisture is low, the sample quality should be taken more.
Solid samples should be grind to fine powder as far as possible for
extraction of moisture.)

8.2) Press START key.

The display will appear as-

ADD SAMPLE

EX.TIME: 10 secs.

8.3) SAMPLE SHOULD BE ADDED AFTER PRESSING THE `START’ KEY


ONLY.

8.4) When the EX.TIME decrements to 00 seconds.

The dispensing unit will start adding the K.F Reagent and on the display the
counting will start.

8.5) The display will appear as-

TITRATION STARTED
00.10 ml

CONF.TIME = 20 secs.

14
Second line of the display shows the consumption of K/F Reagent in ml. When
the moisture is neutralized, the counting will stop, conf. time will start
decrementing. If on decrementing the time, the moisture still remains even
after the time reaches `00’, the dispensing unit will start again and will add the
K/F Reagent. The counts will increase according. When the complete moisture
is neutralized, the conf. time will decrement to `00’ seconds and the audio
signal will indicate that the end point is reached.

8.6) The display should appear as-

K.F.R. READING

02.88 ml.

Taking for granted, the titre factor of reagent = 6.25 18 mgs = 6.25 X 2.88.

8.7) To find out % and PPM.

8.8) Enter the sample quantity.

Press 9 key.
SMPL QUANTITY

8.9) The display will appear as-

SAMPLE QUANTITY

00000003 gm/ml
PRESS ENTER TO CONT.

8.10) (The quantity which is showing on the display may be of last test).
To enter the weight = 150 mgs, enter the weight in gms i.e.0.150 gms.

8.11) Press [0] [.] [1] [5] [0]

The display will indicate as-

SAMPLE QUANTITY

0000.150 gm/ml.
PRESS ENTER TO CONT.

Press ENTER key.

15
8.12) The display will appear as-

K.F.R. READING

02.88 ml.

8.13) Press 7 % key.


PPM

The display will appear as-

WAIT
Calculating % and PPM

8.14) and the display will change over to-

% = 12.000
PPM = 120000.000
Mg of H2O = 18.0000

PRESS ENTER TO EXIT

Press ENTER key.

8.15) The display will appear as-

K.F.R. READING

02.88 ml.

8.16) TO TEST THE LIQUID SAMPLE.


Example- Methanol: Add 10 ml, as sample.

8.17) Press START key.

The display will appear as-

ADD SAMPLE

EX.TIME = 10 secs.

16
8.18) NOTE: SAMPLE SHOULD BE ADDED AFTER PRESSING `START’ KEY.

When the CONF.TIME decrements to 00 secs, the dispensing unit will get `ON’
and start adding the K/F Reagent.

TITRATION STARTED

00.10 ml.

CONF.TIME = 20 secs.

8.19) When the total moisture is neutralized, CONF.TIME decrements to `00’ seconds.

The display will appear as-


TITRATION STARTED

00.56 ml.

CONF.TIME = 00 secs.

(Quantity of reagent 00.56 is taken as example).

The audio signal will indicate the end point is established.

8.20) The display will indicate as-

K.F.R. READING

00.56 ml.

8.21) TO FIND OUT % & PPM.


To enter the SMPL QTY = 10 ml.

8.22) Since the SMPL QTY added is ml, it is necessary to enter the density of solvent,
methanol density such as 0.793

8.23) Press 9 SMPL key.


QTY

The display will appear as-

SAMPLE QUANTITY

0000003 gm/ml.
PRESS ENTER TO CONT.

The line indicating the gm/ml of sample quantity may be of last check.

17
8.24) To enter the new value, press [1] [0].

The display will indicate as-

SAMPLE QUANTITY

0000010 gm/ml.
PRESS ENTER TO CONT.

Press ENTER key.

8.25) The display will appear as-

K.F.R. READING

00.56 ml.

8.26) To enter the density, i.e. = 0.793, press 8 key.


DENSITY

The display will appear as-

DENSITY

0000001 kg/L
PRESS ENTER TO CONT.

Second line of the display is indicating the density as 1 (which is the set value).

8.27) To enter the new density i.e. 0.793, press [0] [.] [7] [9] [3].

The display will appear as-

DENSITY

0000.793 mg/L
PRESS ENTER TO CONT.

Press ENTER key.

18
8.28) The display will appear as-

K.F.R. READING

00.56 ml.

8.29) Press 7 % key.


PPM

The display will appear as-

WAIT
CALCULATING % and PPM

8.30) The above message will appear for few seconds and will change to-

% = 0.044
PPM = 440.000
Mg of H2O = 3.5000

PRESS ENTER TO EXIT

Press ENTER key.

8.31) The display will appear as-

K.F.R. READING

00.56 ml.

To test the next sample, press START key and follow the procedure as per
Paragraph 8.2

** IF SOME TIME IS LOST, THEN THE FRESH END POINT SHOULD BE


OBTAINED AND THEN PRESS THE `START’ KEY.

9.0) SOLVENT BLANK (i.e. Dilution of sample in a solvent)

9.1) Example: If the sample is having low moisture, it is not possible to add large
quantity of sample or if the sample contains high % of moisture like
30% or more. It requires to add very small quantity of sample. In
this case, the dilution technique is suitable.

19
9.2) Example: For moisture of order of 0.1%, the sample quantity required is atleast
10 gms, so that the mgs of H2O available is 10 mgs. For such
samples, the dilution technique is suitable.

9.3) Dissolve the sample quantity 10 gms in 20 ml of methanol.

9.4) It is necessary to determine the moisture in the methanol also. i.e. Blank
Reading of methanol only known as `Solvent Blank’.

9.5) Add 1 ml of methanol in the titration vessel.

(If time is lost, obtain the fresh end point by pressing the START key and wait
till the audio signal indicating fresh end point, before adding the methanol.)

9.6) Press START key and follow the procedure as paragraph 8.2

9.7) Suppose the reading of K/F Reagent to neutralize 1 ml of methanol = 0.05 ml.

9.8) The display will appear as-

K.F.R. READING

00.05 ml

9.9) To enter the reading into solvent blank mode,

Press 5 key.
SOLVENT BLANK

The display will appear as-

SOLVENT BLANK

0000000 ml
PRESS ENTER TO CONT.

9.10) To enter the volume, press [0] [.] [0] [5].


The display will appear as-

SOLVENT BLANK

00000.05 ml.
PRESS ENTER TO CONT.

Press ENTER key.

20
9.11) The display will appear as-

K.F.R. READING
00.05 ml.

9.12) Now add 1 ml of diluted sample (without loosing any time gap). (Remember
sample is diluted by adding 10 gms of sample in 20 ml of methanol).

9.13) Press START key and follow the procedure as per paragraph 8.17 to 8.20

The display will appear as-

K.F.R. READING

01.55 ml.

Taking for granted, the consumption of K/F Reagent required for 1 ml of diluted
sample.
9.14) To enter the sample quantity, i.e. 0.500 gms.

(Since 20 ml of methanol contains= 10 gms of sample, 1 ml of methanol


contains= 0.500 gms of sample.)

9.15) Press 9 key.


SMPL QTY

The display will appear as-

SAMPLE QUANTITY
0000010 gm/ml.
PRESS ENTER TO CONT.

The third line on the display may be of last test.

9.16) To enter the new weight, press [0] [.] [5] [0] [0].

The display will appear as-

SAMPLE QUANTITY

0000.500 gms/ml.
PRESS ENTER TO CONT.

21
9.17) Press ENTER key.

The display will appear as-

K.F.R. READING

01.55 ml.

9.18) To find out % and PPM, press 7 % key.


PPM

(Formula % = T.F X (Reading – Solvent Blank Reading) X 100


Weight of the sample in gms.

% = 6.25 X (1.55 – 1.05) X 100


0.500
9.19) The display will appear as-

WAIT
CALCULATING % AND PPM

9.20) This message will remain for few seconds and change to-

% = .625
PPM = 6250.000
Mgs of H2O = 3.1250

PRESS ENTER TO EXIT

9.21) Press ENTER key.

The display will appear as-

K.F.R. READING

01.55 ml.

10) EXTRACTION TIME 4 EX


TIME

10.1) In most of the liquid samples, the moisture is extracted by the methanol in the
titration vessel, as soon as it is added. In the case of high viscous liquids and
from some of the solid samples, moisture may not be extracted immediately. In
such samples, more extraction time is necessary to extract the moisture.

22
10.2) During this extraction time all functions are stopped. Only stirring is kept `ON’
to extract the moisture. When `EXTRACTION TIME’ is over, the dispensing unit
will start adding K/F Reagent.

10.3) The `EXTRACTION TIME’ is set to `10’ seconds, but this can be varied from 1
second to 240 seconds as per requirement, by following process.

10.4) The display is indicating as- (For example)

K.F.R. READING

00.56 ml.

Second line is showing the reading of K/F Reagent may be of last test.

10.5) Press 4 EX key.


TIME

The display will appear as-

EXTRACTION TIME
0010 Secs.

PRESS ENTER TO CONT.

The second line of display is showing set value of 10 seconds.

10.6) To change the time, say 20 seconds, press [2] [0].

The display will indicate as-

EXTRACTION TIME
0020 Secs.

PRESS ENTER TO CONT.

10.7) Press ENTER key.

The display will indicate as before-

K.F.R. READING

00.56 ml.

23
10.8) To cancel the Ex-time of 20 seconds and go to `SET VALUE’, it can be done by
pressing the CE key or, can over write.

10.9) Example: EXTRACTION TIME

0020 Secs.

PRESS ENTER TO CONT.

Press CE key. Or Press [1] [0].


CLEAN

10.10) The message will appear as-

EXTRACTION TIME

00.10

PRESS ENTER TO CONT.

10.11) Press ENTER key.

The display will appear as before-

K.F.R. READING

00.56 ml.

11) PRINTER
An 80 column dot matrix printer can be attached to the instrument. Printer port
is provided at the rear. Attach the printer, load the paper and switch `ON’ the
printer.

While testing the samples, after calculations, if the printer is put `ON’,
immediately the printer will print the entire data. If one wants to take more
prints or if the printer is not connected while test is `ON’, he can connect the
printer after the calculations and get the entire print by pressing `PRINTER’ key.

24
12) `CLEAN’ Key.
It is necessary to clean the system (dispensing unit) after finishing the days
work.

Fill methanol in the second reservoir bottle of 250 ml, amber colour. Lift the
(glass) Adapter from the K/F Reagent bottle. Press `CLEAN’ key and attach the
adapter to the methanol bottle. The dispensing unit will start sucking the
methanol from the bottle. When clear drops from the dispensing tube start
falling in the titration vessel, just detach the tube from the glass adapter, the
remaining methanol in the dispensing tube will empty into the titration vessel
and after few minutes the system will stop automatically.

PROCESS OF CLEANING

Press CLEAN key.

The display will appear as-

Are you ready


For cleaning
Any key to EXIT
Enter to continue

Press ENTER key.

The message will appear as-

Remove Glass Adapter


From K/F Reagent bottle
And connect to
Methanol Bottle

Press ENTER key.

Connect Glass
STOPPER
TO
K/F Reagent Bottle

Press ENTER key.

WAIT
CLEANING STARTED

PRESS CLEAN TO STOP

25
The dispensing unit will start sucking the methanol. To `Stop’ in between, press
`STOP’ key again. OR When clear drops of methanol from the dispensing tube
start falling in the titration vessel, lift the adapter from the reservoir, so that air
will enter and remaining methanol in the tube will empty in the titration vessel
and after few minutes the system will stop automatically.

The display will appear as-

VEEGO/MATIC-MD

13) BATCH NO 1 BAT


NO

To enter batch number, e.g: as 1 2 3 4, press BATCH NO key.

The display will appear as-

BATCH NUMBER
0000

Press ENTER to cont.

Press [1] [2] [3] [4]

The message will appear as-

BATCH NUMBER
1234

Press ENTER to cont.

Press ENTER key.

The message will appear as-

VEEGO/MATIC-MD

26
14) GENERAL PRECAUTIONS:
Never drop magnetic rotor in reaction beaker with the beaker fixed on the
machine. It is sure to break the beaker due to strong pull of the magnet fitted
inside the machine. Never tighten the nuts of beaker clamp excessively as it may
crush the ground edge of the beaker or deform the beaker holding ring.

All components in the chassis are selected and adjustments carefully done at our
works and sealed. Each instrument is sent out after rigorous testing. For any
problem arising in regular working, consult us before attempting any repairs.

15) INAPPROPRIATE SAMPLES.

It may also be noted that the K/F Reagent does not react with most of the
materials. However, following compounds do react with this reagent and hence
cannot be tested for moisture estimation.

L-Ascorbic Acid. Hydrazine Salts and their substitutes.


Mercapeteirs. Alkali Carbonates & Bicarbonates.
Boric Acid & Boric Oxide. Alkali Sulphites & Pyrosulphites.
Cupric & Ferric Salts. Sodium Tetra-Borates & Thiosulphates.
Metal Oxides & Hydroxides. Sodium Arsenates & Arsenates.
Stennous Chloride. Aldehydes & Ketonic group.

16) MAINTENANCE & CARE OF THE INSTRUMENT.


16.1) The most important care that the instrument needs is cleanliness. Do not spill
any drop of the solution of the cabinet. If at all any drop falls on it, it can be
fairly cleaned by a little soft piece of cloth or cotton moist with acetone or
solution of Sodium-thio-sulphate. This is possible only if it is tried immediately.
The chassis is having a number of settings on it. All these are carefully set
before the instrument is supplied. DO NOT DISTURB ANY OF THE CONTROL AS
THEY ARE CRITICAL.

16.2) Strictly avoid the tips of the sensing electrodes to come in contact with the
grease. It may render them inactive. They also should not be touched by
hand.

16.3) The syringe with the needle should be immediately cleaned and dried after the
work is over, in order to avoid permanent sticking of plunger.

16.4) Never insert the magnetic stirring rotor in the vessel when it is kept on the
machine. The pull of the powerful magnet inside the machine will break the
vessel.

27
17) REPLACING THE TUBE OF THE DISPENSER.
17.1) Disconnect the cable from the mains supply.

17.2) Remove the tubes from the INLET & OUTLET of the dispenser and remove the
solution bottle crate.

17.3) Unscrew the four holding screws and remove the dispenser cover. The
dispenser tube is fitted in a rectangular housing. This housing is mounted on a
metal plate by four screws. (DO NOT DISTURB THIS SETTING AS THIS IS
DONE VERY PRECISELY.)
17.4) Remove the four nuts which are fitted on the four corners of the rectangular
housing. The top portion of the housing will come out along with Teflon nozzles
and the dispenser tube.

17.4) Take out the nozzles from the housing and remove the tube from both nozzles
by pulling out carefully. Pull the white colour Teflon spool from the housing.

17.5) Clean the inside part of the dispensing housing (which is fitted to the plate) if
any spillage of K/F Reagent is there.

17.6) Check that the `U’ shape tension springs are in-tact. (Which are fitted to both
side of the spool.)

17.7) First fit the spool. Insert the spool by pressing the roller inside and see that the
pin enters the slot (fitted on the motor shaft).

17.8) Spare silicon tubes of standard length (92 mm to 95 mm) are supplied along
with the instrument.

17.10) Connect the nozzles to both ends of the silicon tube.

17.11) Place the nozzles into the cavity provided on the part of the housing (which is
fixed permanently on the metal plate). See that the tube gets wound over the
Teflon rotor.

17.12) Place the top portion of the housing on the fixed portion of the housing such
that both Teflon nozzles get fixed in the cavity of the housing.

17.13) Rotate the Teflon rotor by hand and make sure that the tube is free inside the
housing without getting pinched in between two parts of the housing.

17.13) Fit the four screws and again check that the tube is free inside the housing.
Fix back the cover of the dispenser with the four holding screws.

17.15) Connect the tubes to the INLET & OUTLET of the dispenser and fit back the
solution bottle crate.

17.16) Now the instrument is ready for further testing.

28
18) SOLUTION ERROR
The solution error message `SOLErr’ indicates the problems regarding
solutions. This message if appears, while titrating the initial moisture in
methanol itself indicates that either methanol contains high percentage of
moisture or the K/F Reagent is very old deteriorated (i.e. the factor of K/F
Reagent must be below 4) or K/F Reagent and Methanol both are faulty.
While `SOLErr’ appears on the display, the alarm also sounds ON/OFF
intermittently.

Check the following points when solution error appears on the display.

18.1) The quality of methanol.


Whether it is K/F Grade or not otherwise replace it with fresh K/F Grade
Methanol.

18.2) The quality of K/F Reagent.


Whether it is fresh or not otherwise replace the K/F Reagent with fresh
K/F Reagent.

18.3) Quantity of K/F Reagent in reservoir.


Whether enough K/F Reagent is in the reservoir otherwise add some K/F
Reagent into reservoir.

18.4) Connection of Pt-Sensor Electrodes.


Check connection of Pt-Sensor (Electrodes). If not proper, re-fit it.

18.5) Adapter fitting.


Whether the adapter is properly fitted to the reservoir and greased otherwise
fit it properly and grease it properly.

18.6) Condition of delivery tube.


Whether there is any fold in the delivery tube. Set the tube and replace the
tube if necessary.

18.7) Condition of Dispensing Tube.


Whether leakage is in dispenser system. (i.e. check whether the solution is
coming out of the drainage provided on the rear panel of the instrument.) If
some solution is coming out from drainage tube, it indicates that the tube
inside the dispenser is burst, refer to paragraph `REPLACEMENT OF TUBE’.

18.8) The message will appear as-

SOLUTION ERROR

ENTER TO CONTINUE

29
The intermittent audio signal will indicate solution error message is appearing
on the display.

18.9) Press ENTER key.

The message will appear as-

CHK - METHANOL
CHK - BOTTLE EMPTY
CHK - KFR REAGENT
ENTER TO CONTINUE

18.10) Press ENTER key.

The message will appear as-

CHK CONNECTING TUBE


CHK PT SENSOR
CHK DISPENSING TUBE
ENTER TO RE-START

18.11) User should take corrective measure as per the instructions.

18.12) And press ENTER key.

The message will appear as-

VEEGO/MATIC-MD

18 : 19 : 45

30
ADDITIONAL INSTRUCTIONS
MODEL
VEEGO/MATIC – MD
The instrument is having the facility to Validate and Calibrate the flow of the
dispensing pump. Pressing CLEAR key can do this.

DISPENSER CALIBRATION:

Fill sufficient amount of distilled water into the reservoir and connect it to the ‘INLET’
of the dispenser. Connect the ‘OUTLET’ of the dispenser to a small beaker.

Allow the dispenser to run for sometime so that the Inlet and Outlet tubes are filled
with water. This can be done by running the clean cycle of the dispenser.

Thus the dispenser is now ready for calibration after air bubble is removed. Now weigh
the beaker accurately and note down its weight. Call this as ‘B’ g. (e.g. B = 12.56 g)

On pressing the ‘CLEAR’ key the display will show the message

DO YOU WANT TO
VALIDATE DISPENSER
ANY KEY TO EXIT
ENTER TO CONTINUE

If you want to continue with Validation or Calibration of the dispenser, press ENTER
otherwise press any key to exit. On pressing the ENTER key the display will show the
message

DISPENSER READY

ANY KEY TO EXIT


ENTER TO CONTINUE

If the dispenser is ready after removing air bubbles etc., then to continue with
Validation or Calibration of the dispenser, press ENTER otherwise press any key to exit.
On pressing the ENTER key the display will show the message

SELECT MODE
VALIDATION / CALIBRATION
SELECT TO CHANGE
ENTER TO CONTINUE
31
Observe that the message ‘VALIDATE’ is blinking, on pressing the SELECT key the
message ‘CALIBRATE’ will blink. Press SELECT to choose the either of the modes.
Press SELECT to choose ‘CALIBRATE’ mode. Observe that on pressing the SELECT key
the message ‘CALIBRATE’ is blinking. Now press ENTER to continue. On pressing the
ENTER key the display will show the message

DISPENSER READY

ANY KEY TO EXIT


ENTER TO CONTINUE

If the dispenser is ready after removing air bubbles etc., then to continue with
Calibration of the dispenser, press ENTER otherwise press any key to exit. On pressing
the ENTER key the display will show the message

ENTER REQUIRED VOLUME


00.00 ml

PRESS ENTER TO CONTINUE

Now enter the required volume to be dispensed for calibrating the dispenser, Say
10.00 ml. After entering the required volume the display will show

ENTER REQUIRED VOLUME


10.00 ml

PRESS ENTER TO CONTINUE

Now press ENTER to continue the calibration. On pressing the ENTER the display will
show

PLACE THE CYLINDER


AND

ENTER TO CONTINUE

32
Now place the beaker (or cylinder) just below the delivery tip and press ENTER. The
display will show

WAIT
ADDING LIQUID

00.00 ml

Observe that the dispenser is adding the water into the beaker and the display
indicates amount of water being dispensed. After 10.00 ml water is dispensed, the
dispenser stops and the display shows the message

ENTER DISPENSED VOLUME


00.00 ml

PRESS ENTER TO CONTINUE

Now weigh the beaker and note down its weight. Call it as ‘A’ g (e.g. A=22.26 g). The
difference (A-B) will be weight of the water dispensed i.e. volume of water. Thus the
volume dispensed is 9.70 ml. Now on entering the volume dispensed as 09.70 ml the
will show.

ENTER DISPENSED VOLUME


09.70 ml

PRESS ENTER TO CONTINUE

After entering the volume press ENTER. The display will show.

ENTER DISPENSED VOLUME


09.70 ml
ANY KEY TO CHANGE
PRESS ENTER TO CONTINUE

33
To edit the dispensed volume, press any key so that the volume can be edited.
Otherwise press ENTER to confirm. On pressing the ENTER key the display will show

ARE YOU READY FOR


NEXT RUN
ANY KEY TO ABORT
ENTER TO CONTINUE

The same experiment is repeated thrice and the average volume is calculated. To
continue with the calibration press ENTER key and repeat the experiment again. Each
time calculate the dispensed volume and enter it properly. If you do not want to
continue with calibration further, press any key to abort. In that case the average of
whatever calibration is performed will be calculated.

After the calibration is over the display will show the message with an audio signal for
few seconds.

CALIBRATION OVER

The message will be cleared automatically after few seconds.

DISPENSER VALIDATION:

Fill sufficient amount of distilled water into the reservoir and connect it to the ‘INLET’
of the dispenser. Connect the ‘OUTLET’ of the dispenser to a small beaker.

Allow the dispenser to run for sometime so that the Inlet and Outlet tubes are filled
with water. This can be done by running the clean cycle of the dispenser.

Thus the dispenser is now ready for validation after air bubble is removed. Now weigh
the beaker and note down its weight. Call this as ‘B’ g. (e.g. B = 12.56 g)
On pressing the ‘CLEAR’ key the display will show the message

DO YOU WANT TO
VALIDATE DISPENSER
ANY KEY TO EXIT
ENTER TO CONTINUE

34
If you want to continue with Validation of the dispenser, press ENTER otherwise press
any key to exit. On pressing the ENTER key the display will show the message

DISPENSER READY

ANY KEY TO EXIT


ENTER TO CONTINUE

If the dispenser is ready after removing air bubbles etc., then to continue with
Validation of the dispenser, press ENTER otherwise press any key to exit. On pressing
the ENTER key the display will show the message

SELECT MODE
VALIDATION / CALIBRATION
SELECT TO CHANGE
ENTER TO CONTINUE

Observe that the message ‘VALIDATE’ is blinking, Now press ENTER to continue for the
Validation of the dispenser. On pressing the ENTER key the display will show the
message

DISPENSER READY

ANY KEY TO EXIT


ENTER TO CONTINUE

If the dispenser is ready after removing air bubbles etc., then to continue with
Validation of the dispenser, press ENTER otherwise press any key to exit. On pressing
the ENTER key the display will show the message.

ENTER REQUIRED VOLUME


00.00 ml

PRESS ENTER TO CONTINUE

35
Now enter the required volume to be dispensed for validating the dispenser, Say 10.00
ml. After entering the required volume the display will show

ENTER REQUIRED VOLUME


10.00 ml

PRESS ENTER TO CONTINUE

Now press ENTER to continue the. On pressing the ENTER the display will show

PLACE THE CYLINDER


AND

ENTER TO CONTINUE

Now place the beaker (or cylinder) just below the delivery tip and press ENTER. The
display will show

WAIT
ADDING LIQUID

Observe that the dispenser is adding the water into the beaker and the display
continues to show above message. After 10.00 ml water is dispensed, the dispenser
stops and the display shows the message

CHECK DISPENSED VOLUME

PRESS ENTER TO CONTINUE

Now weigh the beaker and note down its weight. Call it as ‘A’ g (e.g. A=22.52 g). The
difference (A-B) will be weight of the water dispensed i.e. volume of water. Thus the
volume dispensed is 9.96 ml.

36
If necessary repeat the validation three times. Observe that the readings obtained vary
by not more than +/- 0.20 ml to the corresponding 10-ml volume.

AFTER USING THE


DISPENSER WITH
WATER, RINSE IT
WITH METHANOL

CALIBRATION ERROR:
If the flow of the dispenser is too less or too high, then there is likely to have an error
in the dispensing system. In case the volume is not entered properly, the display may
show the following message with a continuous audio signal.

CALIBRATION ERROR

PRESS ENTER TO CONTINUE

This indicates that there is an error in the calibration. The above message will be
displayed with a continuous audio alarm. On pressing the enter key the display will
show the checklist of the few of the probable reasons.

CHECK DELIVERY TUBES


CHECK SPRINGS/NOZZLES
CHECK DISPENSING TUBE
PRESS ENTER TO CONTINUE

Please check the above and take the corrective action. On pressing the ENTER key the
display will show the message.

RECALIBRATE
DISPENSER

PRESS ENTER TO CONTINUE


After taking the corrective measures recalibrate the dispenser.

37
CALIBRATION FREQUENCY:

It is recommended to calibrate the dispenser once every month. Also it should be


calibrated whenever the dispensing tube is changed.

IT IS NOT NECESSARY
TO CALIBRATE
DISPENSER DAILY

NOTE:

The validation and calibration of the dispenser can be done with any solvent like
Methanol or K. F. Reagent also. In that case use any ‘Certified Class A Cylinder’. The
method explained above is suitable and accurate provided a balance is available.

38

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